?fining of tall oil



. specification and the appended claim.

Patented June '27, 1944 John D. Jen kins, Milwaukee, Wis.',' assignor to, 4 Pittsburgh Plate Glass Company, Allegheny County, Pa., a corporation of Pennsylvania No Drawing. Application December 19, 1941,

Serial No. 423,626

1 Claim. (Ci. zoo-91.5)

The present invention relates to the treatment of tall oil and it hasparticularrelation to its treatment for purposes of separating it into components.

One object of the invention is to provide a simple and economical process of treating tall oil whereby resin acids can be separated from fatty acids, sterols and the like, to obtain fractions better adaptedfor use in resin making, soap making and other arts than is the impure mix-- tureconstituting the original mixture.

This and other objects of the invention will be apparent from consideration of the foilowin Tall oil is obtained in large quantitiesin the paper industry from the manufacture of paper If fu'rfural is employed the saturation point is probably about '4 or at ordinary atmospherictemperatures. If diacetone alcohol is employed,

it may ;contain about 11% of water.

The ratio of tall oil to solvent is-variable; but

in the case of the monomethyl' ether of ethylene;

glycol its] concentration in the solvent is about 2 to 50%.

In order to eifect crystallization, the solution may be all wed to stand quietly at room temperature, r it may be stirredoccasionally to permit crystallization to occur. Crystallization is permitted to continue until a suilicient amount of pulp by the sulfate process. The major constituents of the oil comprise resin acids, fatty acids and some non-acid constituents, such as ste'rols Some of these constituents are, if.in pure state, of great value, but in thecomplex association in which they exist. in tall oil they have but little value, and for that reason, use of tall oil, up to the present time, has been very limited. 1

The present invention contemplates the provision of a process of separating resin .acids from of water and the solution is then chilled or otherwise subiected to conditions to effect a crystal lization of the resin acids. Th crystallized niaterial can then be removed by filtration or centrifugation, decantation orf'similar methods to obtain a solution consisting largely of fatty acids and sterols. 4

the resin acids have thus been precipitated. If desired, the crystallizationmay be promoted by chilling the solution or by evaporating away the solvent. The crystals can be separated at any convenient manner, for example, by decantaand the like. The following is a typical composition:

Per cent Fatty acids.. -50 to 60 Resin acids 34 to 48 Non-acids .6to,

tion, centrifugation or the like methods. Residsolvent and fatty acids can be removed by washing with. water or the like. The crystals consist essentially of the resin acids which can be used in the preparationiof soaps, and for other purposes.

The" fatty acids and the non-acids including sterolsand .the like are retained in the solvent medium and may be recovered by evaporating the latter to dryness, orby extracting 'it with petroleuni naphtha. If it is desired to separate the non-acid constituents including the sterols from the fatty acids, the; latter may be saponifled with tall oil, in which the oillismerely dissolved in r a polar solvent containing a considerable amount In the practice of the invention,-various polar I solvents may be employed as the solvent medium considered that monomethyl ether of ethylene slycol is from all angles highly meritorious. Still other polar solvents including furrural and dipotassium or sodium hydroxide 'inwater solution and the non-acids then extracted by means 'of ether or naphtha. The products of saponifl- ;cation may be acidified in order to liberate the free acids which can then be employed for vari- Oils purposes including the manufacture of soaps". resins and the. like.

Alkyd type resins may be prepared by admixing glycerol or glycol or a mixture of the two with recovered fatty acids or recovered resin acids and phthalic anhydride.

, phthalic anhydridetofatty acids may be apfor thetalloil. However, itisatthe present time Pmximately and the W591 phthall within the purview'ofthe invention.- For best results. solvent .media are admixed with waterin'suitable-P mrtion. In thecase of the tained. The tall oil a monoethyl ether ofethylene glycol, the water ratio, preferablyfls withina range of 20 to 80%,

anhydride and free acid should be approximately molecularly equivalent to the polyhydroxy alcohol. The mixture, is heated to reaction temacetcne alcohol are, also, considered as being Derature, as evidenced byevolution of water.

The reaction is continued for several hours, or until desired consistency of the product is obor resin acids.

Resin acids can be saponified with caustic sodabased upon the content of the monomethyl ether. added to a w ter s spension of paper pulp. B

paper sizes The ratio of cids may be either fatty acidiivinztheeoeporbyaddiugalumasizeis precipitated upon the pulp.

The sterols may be recovered from the nonacid rractions by appropriate treatment and are suitable for use as sources of pharmaceuticals,

and other uses. 4

. The forms 01 the invention herein described are to be considered merely as exemplary. It willbeapparentto thoeeskilledintheartthat numerousmodifications may be made therein without departure from. the spirit or the invention or the scope of the appended claim.

from the liquid residue.

wnstraaimp: a Aprocessot eeperatinlreeinecids iromtell .oil.whichproceeeeomprisesdiasolvinltheoilina polar solvent selected iron the group consistin: of mono methyl ether of ethylene glycol, and

diacetone alcohol, the solvent containing 9.1 sub stantial amount of water. crystallining out the resin acids from the solution and separating them 6 JOHN 11 JENKINS. 

